関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | 1-[4-(4-Aminophenyl)piperazin-1-yl]ethan-1-one | HCID 736269 | — |
| 反応物 | 2-chloro-4-(methylthio)-7H-pyrrolo[2,3-d]pyrimidine | HCID 57990275 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(4-(4-(4-(methylthio)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino)phenyl)piperazin-1-yl)ethanone | HCID 69023137 | 48.7% |
反応手順
A mixture of 2-chloro-4-(methylthio)-7H-pyrrolo[2,3-d]pyrimidine (484 mg, 2.43 mmol), 1-(4-(4-aminophenyl)piperazin-1-yl)ethanone (645 mg, 2.95 mmol) and trimethylsilyl chloride (0.500 mL, 3.95 mmol) in nBuOH (10 mL) was heated at 116° C. for 48 h. After cooling down, H2O and EtOAc were added. The organic phase was separated, washed with 5% NaHCO3, dried over Na2SO4, concentrated in vacuo to give 1-(4-(4-(4-(methylthio)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino)phenyl)piperazin-1-yl)ethanone as a solid (453 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08258144B2 |
|---|
| 出典データセット | uspto-grants-2012_09 |
|---|
| ORD ID | ord-9ab068c6bbaa4934b1646ed25d2749af |
|---|
| 出典メモ | uspto-grants-2012_09 |
|---|
